Preparation method of solubilizing agent

A technology of solubilizer and organic solvent, applied in the field of preparation of solubilizer, can solve problems such as uneven purity, influence effect, etc., and achieve the effects of simple operation, small pollution, and reducing the difference of results

Inactive Publication Date: 2018-09-07
辅创科技(宜昌)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the current research results have shown the excellent value o...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 150g of commercially available TPGS (containing polyethylene glycol 15wt%, active ingredient 127.5g, vitamin E succinate 0.71g in the active ingredient), add it to 450g ethyl acetate, heat to dissolve, add 20wt% saline 450g, 40℃ Insulate and stir evenly, let stand to separate layers, wash the organic layer twice according to the law, take the organic layer, add 20g of calcium oxide, heat and stir at 40°C for 3 hours, filter, evaporate the solvent under reduced pressure to obtain 121.3g of PEG-TPGS (vitamin E Succinate 0.67g), using an ELSD detector (evaporative light scattering detector), the liquid phase detection PEG content is 0.35%, and the active ingredient yield is 95%.

Embodiment 2

[0026] Take 150g of commercially available TPGS (containing 20wt% of polyethylene glycol, 3.9wt% of vitamin E succinate, 120g of active ingredients), add it to 600g of butyl acetate, heat to dissolve, add 50g of 15wt% saline, 60°C Insulate and stir evenly, stand and separate layers, wash the organic layer five times according to the law, take the organic layer, add 80 g of anhydrous sodium sulfate, heat and stir at 60 ° C for 3 hours, filter, and evaporate the solvent under reduced pressure to obtain 115.5 g of PEG-TPGS. The PEG content is 0.23%, and the yield is 96%.

Embodiment 3

[0028] Take 150g of synthesized TPGS (containing 6% polyethylene glycol, active ingredient 141g), add it to 500g toluene, heat to dissolve, add 300g of 25wt% brine, keep stirring at 30°C and keep it to separate layers. Wash three times with water, take the organic layer, add 60g of alumina, keep stirring at 30°C for 3 hours, filter, and evaporate the solvent under reduced pressure to obtain 134.4g of PEG-TPGS with 0.32% PEG content and a yield of 90.5%.

[0029] Separation and comparison

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PUM

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Abstract

The invention discloses a preparation method of a solubilizing agent, and belongs to the technical field of solubilizing agents. The method comprises the steps that to-be-purified vitamin E-polyethylene glycol-succinate is dissolved in an organic solvent, heated to be dissolved, washed for 1-5 times with saline water, dried with a drying agent after washing, and filtered after drying, the organicsolvent is steamed out to obtain vitamin E polyethylene glycol succinic acid ester with low content of polyethylene glycol; the organic solvent is selected from ethyl acetate, butyl acetate or methylbenzene; the content of the polyethylene glycol in the to-be-purified vitamin E-polyethylene glycol-succinate is 5-30% by weight, and the content of the vitamin E-succinate is less than 0.5% by weight.The preparation method of the solubilizing agent has the advantages that simple technology and low cost are used to purify the crude vitamin E-polyethylene glycol-succinate, the operation is simple,no special equipment is needed, the polyethylene glycol in the product can be effectively removed and controlled in a certain range, and the vitamin E succinate is reserved.

Description

technical field [0001] The invention relates to the technical field of solubilizers, in particular to a preparation method of a solubilizer, in particular to a purification method for making the purity of polyethylene glycol less than 0.5% and virtually no loss of vitamin E polyethylene glycol succinate. Background technique [0002] Vitamin E polyethylene glycol succinate (TPGS) is a water-soluble derivative of natural vitamin E, which is obtained by the esterification reaction of hydrophilic polyethylene glycol (PEG) and lipophilic vitamin E succinate , At the same time, it has the physiological activity of PEG and vitamin E. It is a white or light yellow waxy solid at room temperature, with a melting point of 37-41 ° C. It can exist stably in the air. TPGS was first developed and marketed by Eastman Company of the United States in 1950. Because it has both lipophilic groups of vitamin E and long-chain hydrophilic groups of polyethylene glycol, it has the property of surfa...

Claims

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Application Information

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IPC IPC(8): C08G65/30
CPCC08G65/30
Inventor 杜诗
Owner 辅创科技(宜昌)有限公司
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